Abstract

HIPPIE is a soft X-ray beamline on the 3 GeV electron storage ring of the MAX IV Laboratory, equipped with a novel ambient-pressure X-ray photoelectron spectroscopy (APXPS) instrument. The endstation is dedicated to performing in situ and operando X-ray photoelectron spectroscopy experiments in the presence of a controlled gaseous atmosphere at pressures up to 30 mbar [1 mbar = 100 Pa] as well as under ultra-high-vacuum conditions. The photon energy range is 250 to 2200 eV in planar polarization and with photon fluxes >1012 photons s-1 (500 mA ring current) at a resolving power of greater than 10000 and up to a maximum of 32000. The endstation currently provides two sample environments: a catalysis cell and an electrochemical/liquid cell. The former allows APXPS measurements of solid samples in the presence of a gaseous atmosphere (with a mixture of up to eight gases and a vapour of a liquid) and simultaneous analysis of the inlet/outlet gas composition by online mass spectrometry. The latter is a more versatile setup primarily designed for APXPS at the solid-liquid (dip-and-pull setup) or liquid-gas (liquid microjet) interfaces under full electrochemical control, and it can also be used as an openport for ad hoc-designed non-standard APXPS experiments with different sample environments. The catalysis cell can be further equipped with an IR reflection-absorption spectrometer, allowing for simultaneous APXPS and IR spectroscopy of the samples. The endstation is set up to easily accommodate further sample environments.

Highlights

  • Ambient-pressure X-ray photoelectron spectroscopy (APXPS) is a powerful technique for studying the chemical composition of the interfaces between solids, liquids and gases

  • The endstation is dedicated to performing in situ and operando X-ray photoelectron spectroscopy experiments in the presence of a controlled gaseous atmosphere at pressures up to 30 mbar [1 mbar = 100 Pa] as well as under ultra-high-vacuum conditions

  • The endstation currently provides two sample environments: a catalysis cell and an electrochemical/liquid cell. The former allows ambient-pressure X-ray photoelectron spectroscopy (APXPS) measurements of solid samples in the presence of a gaseous atmosphere and simultaneous analysis of the inlet/outlet gas composition by online mass spectrometry. The latter is a more versatile setup primarily designed for APXPS at the solid–liquid or liquid–gas interfaces under full electrochemical control, and it can be used as an open port for ad hoc-designed non-standard APXPS experiments with different sample environments

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Summary

Introduction

Ambient-pressure X-ray photoelectron spectroscopy (APXPS) is a powerful technique for studying the chemical composition of the interfaces between solids, liquids and gases. At the former MAX-lab (which has evolved into the current MAX IV Laboratory) a new cell-in-cell approach was pioneered (Schnadt et al, 2012) as a natural development of the very early schemes of APXPS instrumentation (Siegbahn & Siegbahn, 1973; Joyner & Roberts, 1979; Joyner et al, 1979; Boronin et al, 1988) In this concept, which was developed simultaneously for X-ray anode-based instruments, the advantages of back-filling and exchangeable cell design are combined to allow quick switching between AP and ultra-high-vacuum (UHV) conditions without compromising sample cleanness.

Design goals and technical details
Beamline
APXPS endstation
Following dynamic phase changes under a graphene cover
Electrochemistry
Findings
Funding information

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